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CN115073122A - Straw aerogel flame-retardant insulation board and preparation method thereof - Google Patents

Straw aerogel flame-retardant insulation board and preparation method thereof Download PDF

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CN115073122A
CN115073122A CN202210685987.XA CN202210685987A CN115073122A CN 115073122 A CN115073122 A CN 115073122A CN 202210685987 A CN202210685987 A CN 202210685987A CN 115073122 A CN115073122 A CN 115073122A
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straw
insulation board
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fibers
aerogel
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汪述平
陆善斌
王洪松
张晶晶
王阳
魏任重
毕海明
陆铜华
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Treezo New Meterial Science and Technology Group Co Ltd
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Abstract

本发明公开了一种秸秆气凝胶难燃保温板及其制备方法。本发明所述秸秆气凝胶难燃保温板由秸秆原料、偶联剂、水溶性硅源、钙源与水混合均匀后铺装预压成型,再经高温高压固型后得到;所述秸秆纤维由长度1~2cm的秸秆长纤维与长度小于1cm的秸秆短纤维复配组成。本发明所述秸秆气凝胶难燃保温板既保留了秸秆的天然纹理,具有较好的装饰效果,也具有轻质高强、表面平整、难燃、轻质无醛、隔热隔音和防霉防蛀等特点。

Figure 202210685987

The invention discloses a straw aerogel flame-retardant thermal insulation board and a preparation method thereof. The straw aerogel flame-retardant insulation board of the present invention is obtained by mixing straw raw material, coupling agent, water-soluble silicon source, calcium source and water uniformly, paving and pre-pressing, and then solidifying at high temperature and high pressure; the straw The fibers are composed of long straw fibers with a length of 1-2 cm and short straw fibers with a length of less than 1 cm. The straw aerogel flame-retardant insulation board of the invention not only retains the natural texture of the straw, has a good decorative effect, but also has the advantages of light weight, high strength, smooth surface, flame retardant, light weight, no formaldehyde, heat insulation and sound insulation and mildew resistance. Anti-moth and other features.

Figure 202210685987

Description

一种秸秆气凝胶难燃保温板及其制备方法A kind of straw aerogel flame retardant insulation board and preparation method thereof

技术领域technical field

本发明涉及一种秸秆气凝胶难燃保温板及其制备方法,属于新型复合纤维板技术领域。The invention relates to a straw aerogel flame-retardant thermal insulation board and a preparation method thereof, belonging to the technical field of novel composite fiber boards.

背景技术Background technique

我国人造板产量和消费量位居世界第一,是人造板生产大国,但林业资源相对短缺,人均森林面积仅为世界人均水平的1/4,木材对外依存度接近50%,森林可采资源少。my country ranks first in the world in terms of production and consumption of wood-based panels, and is a big producer of wood-based panels. However, forestry resources are relatively short. The per capita forest area is only 1/4 of the world's per capita level. The external dependence of wood is close to 50%. few.

我国也是农业大国,农作物秸秆资源丰富,产量巨大,种类多且分布广。将农作物秸秆用于人造板生产领域,既能解决木材短缺的难题,也能促进秸秆资源的利用。my country is also a big agricultural country, with abundant crop straw resources, huge output, variety and wide distribution. The use of crop straw in the field of wood-based panel production can not only solve the problem of wood shortage, but also promote the utilization of straw resources.

公开号CN104724976A的中国专利公开了一种秸秆防火保温板及其生产方法,本发明利用秸秆作为主填充材料,充分利用了秸秆的填充能力强、纤维韧性大和防火保温能力高的特性,在酚醛树脂颗粒、乳胶粉和憎水剂的作用下,生产一种抗弯、抗压和抗折能力强,防火等级高,施工方便和成本低廉的保温板,同时,也解决了农业废弃物的后处理和再利用的问题。该方法采用酚醛树脂作为胶黏剂,会导致样板生产和使用过程中存在甲醛释放的问题,不具备无醛特征。The Chinese Patent Publication No. CN104724976A discloses a straw fireproof thermal insulation board and a production method thereof. The present invention uses straw as the main filling material, and makes full use of the straw's characteristics of strong filling ability, high fiber toughness and high fireproof and thermal insulation ability. Under the action of particles, latex powder and water repellent, a thermal insulation board with strong bending, compressive and flexural resistance, high fire rating, convenient construction and low cost is produced. At the same time, it also solves the problem of post-processing of agricultural waste. and reuse issues. The method uses phenolic resin as the adhesive, which will lead to the problem of formaldehyde release during the production and use of the template, and has no formaldehyde-free feature.

公开号CN103626433A的中国专利公开了一种秸秆保温板及其制备方法,本发明包括芯材层和包覆层两个部分,芯材层主要是通过环氧胶、玉石粉、珠光砂和秸秆压制成型制得,表面包覆层主要利用具有粘接作用的无机胶凝材料均匀的包覆在秸秆板的表层,从而获得一种以秸秆为板材的新型秸秆保温板;该新型秸秆保温板具有快速成型、隔热保温、阻燃、防霉、高强等优异性能。该方法制备的保温板芯表层材质不同,受热膨胀系数不同,可能在使用过程中出现开裂等问题,同时芯层的阻燃性能也有所削弱。The Chinese Patent Publication No. CN103626433A discloses a straw insulation board and a preparation method thereof. The present invention includes a core material layer and a coating layer. The core material layer is mainly pressed by epoxy glue, jade powder, pearl sand and straw. It is prepared by molding, and the surface coating layer mainly uses the inorganic cementing material with bonding function to evenly coat the surface layer of the straw board, so as to obtain a new type of straw insulation board with straw as the board; the new type of straw insulation board has fast It has excellent properties such as molding, heat insulation, flame retardant, mildew resistance, and high strength. The core surface layer of the thermal insulation board prepared by the method has different materials and different thermal expansion coefficients, which may cause problems such as cracking during use, and at the same time, the flame retardant performance of the core layer is also weakened.

公开号CN113084960A的中国专利介绍了一种玉米秸秆板及其制备方式,所述方法利用秸皮软化酶对玉米秸秆长纤维的表面进行刻蚀,暴露出秸皮粗纤维,并使用秸秆具有丰富的孔隙结构,采用纳米纤维素溶液作为增强剂,提高板材强度。此方法处理秸秆的效率较低,且酶反应的条件较为严苛,难以大规模化应用。The Chinese patent publication number CN113084960A introduces a corn stalk board and its preparation method. The method utilizes stalk softening enzymes to etch the surface of the long fibers of the corn stalks to expose the coarse stalk fibers, and uses the stalks with rich stalks. Pore structure, using nanocellulose solution as a reinforcing agent to improve the strength of the sheet. This method has low efficiency in treating straw, and the conditions of enzymatic reaction are relatively severe, so it is difficult to be applied on a large scale.

公开号CN111300565A的中国专利介绍了一种防腐玉米秸秆重组材及其制造方法,所述方法采用间苯二酚改性酚醛树脂为胶黏剂,对玉米秸秆外皮进行疏解、防腐处理。此方法处理制备的复合板不具备阻燃和无醛的特征。The Chinese Patent Publication No. CN111300565A introduces a preservative corn stalk reconstituted material and a manufacturing method thereof. The method uses resorcinol-modified phenolic resin as an adhesive to disperse and anti-corrosion the corn stalk husk. The composite panels prepared by this method do not have the characteristics of flame retardancy and aldehyde-free.

公开号CN112851290A的中国专利介绍了一种利用无机胶黏剂的木材、秸秆纤维板及其制备方法,所述方法制备的秸秆纤维板中纤维含量较低,板材的木质感较差,同时样板密度大,不具备轻质的特征。The Chinese Patent Publication No. CN112851290A introduces a wood and straw fiberboard using inorganic adhesives and a preparation method thereof. The fiber content of the straw fiberboard prepared by the method is relatively low, the woodiness of the board is poor, and the density of the sample board is high. Does not have the characteristics of light weight.

发明内容SUMMARY OF THE INVENTION

针对上述问题,本发明提供了一种秸秆气凝胶难燃保温板及其制备方法,所述秸秆气凝胶难燃保温板具有阻燃、轻质无醛、隔热隔音和防霉防蛀等特点,解决了秸秆可燃性的最大难题,拓宽了秸秆复合板应用领域。In view of the above problems, the present invention provides a straw aerogel flame-retardant thermal insulation board and a preparation method thereof. It solves the biggest problem of straw flammability and broadens the application field of straw composite board.

本发明解决上述问题的方案如下:The scheme that the present invention solves the above-mentioned problem is as follows:

本发明提供了一种秸秆气凝胶难燃保温板,由秸秆原料、偶联剂、无机料与水混合均匀后铺装预压成型,再经高温高压固型后得到;所述无机料包括水溶性硅源及钙源;The invention provides a straw aerogel flame-retardant thermal insulation board, which is obtained by mixing straw raw materials, coupling agents, inorganic materials and water uniformly, then paving and pre-pressing, and then being solidified at high temperature and high pressure; the inorganic materials include: Water-soluble silicon source and calcium source;

上述各组分重量份数如下:The parts by weight of the above-mentioned components are as follows:

Figure BDA0003697888490000021
Figure BDA0003697888490000021

所述水与无机料的质量比为0.8~1;The mass ratio of the water to the inorganic material is 0.8-1;

所述高温高压固型的工艺参数为:温度160~220℃,单位压力为3~10MPa,固型时间为10~30min;The process parameters of the high temperature and high pressure solidification are: the temperature is 160-220°C, the unit pressure is 3-10MPa, and the solidification time is 10-30min;

所述秸秆原料由秸秆长纤维与秸秆短纤维复配组成,其中秸秆长纤维质量占比10%~30%,秸秆短纤维质量占比70%~90%;所述秸秆长纤维的长度1~2cm,秸秆短纤维的长度小于1cm;The straw raw material is composed of long straw fibers and short straw fibers, wherein the long straw fibers account for 10% to 30% by weight, and the short straw fibers account for 70% to 90%; 2cm, and the length of short straw fibers is less than 1cm;

所述秸秆原料的含水率小于10wt%。The moisture content of the straw raw material is less than 10wt%.

所述偶联剂为聚乙烯醇;偶联剂的加入能提高无机胶黏剂与秸秆之间的结合性能,提高界面相容性。The coupling agent is polyvinyl alcohol; the addition of the coupling agent can improve the bonding performance between the inorganic adhesive and the straw, and improve the interface compatibility.

所述水溶性硅源为速溶粉状硅酸钠,模数为2.1~3.4;实际使用时配置成水溶液后的固含量为30%~40%。The water-soluble silicon source is instant powdery sodium silicate, and the modulus is 2.1-3.4; in actual use, the solid content after being configured into an aqueous solution is 30%-40%.

所述钙源为半水石膏;所述钙源为增强剂,钙源的加入能与水溶性硅源反应,生成硅酸钙晶体,从而增强板材的力学性能。The calcium source is hemihydrate gypsum; the calcium source is a reinforcing agent, and the addition of the calcium source can react with the water-soluble silicon source to generate calcium silicate crystals, thereby enhancing the mechanical properties of the board.

本发明采用了硅气凝胶和纤维素气凝胶复合的双胶黏体系。本发明中的水溶性硅源能与秸秆纤维原料均匀混合,在高温高压的过程中,生成二氧化硅气凝胶网络,将秸秆纤维原料粘结在一起;同时,秸秆纤维中的木质素和纤维素也在高温状态下缠绕、反应,形成纤维素气凝胶网络,进一步提高板材的内结合强度。本发明中加入偶联剂聚乙烯醇,能改善硅源与秸秆的界面相容性;加入钙源,能够与硅源、水蒸气在高温高压的条件下反应,生成硅酸钙晶体,在板材内部起到增强筋骨的作用,提高板材的力学性能;同时,水蒸气在高温的条件下蒸发,能在板材中形成气孔,形成复杂的孔道结构,有利于降低板材密度,提高板材保温性能。硅钙体系进一步反应,提高板材的力学强度。The invention adopts a double-adhesive system which is a composite of silicon aerogel and cellulose aerogel. The water-soluble silicon source in the present invention can be uniformly mixed with the straw fiber raw materials, and in the process of high temperature and high pressure, a silica aerogel network is formed to bond the straw fiber raw materials together; at the same time, the lignin and Cellulose is also entangled and reacted at high temperature to form a cellulose aerogel network, which further improves the internal bonding strength of the sheet. Adding coupling agent polyvinyl alcohol in the present invention can improve the interface compatibility between silicon source and straw; adding calcium source can react with silicon source and water vapor under the conditions of high temperature and high pressure to generate calcium silicate crystals, which can be deposited on the board. The inside plays the role of strengthening the bones and improving the mechanical properties of the board; at the same time, the evaporation of water vapor under high temperature conditions can form pores in the board, forming a complex pore structure, which is conducive to reducing the density of the board and improving the thermal insulation performance of the board. The calcium-silicon system reacts further to improve the mechanical strength of the sheet.

本发明采用的秸秆纤维原料选择秸秆长纤维与短纤维的混配,目的是使秸秆纤维与无机胶黏剂混合均匀,促使板材结构紧实,提升板材的力学性能。板材中的秸秆长纤维相互搭接,形成纵横交织的网状结构,能抑制无机凝胶体系中微裂痕的产生及蔓延,提高板材的弹性模量,同时保留了秸秆的自然形貌;秸秆短纤维比表面积大,更容易被水溶性硅源浸润,混合均匀后,填充于板材内部,提高板材的内胶合强度,从而能有效地提高板材的力学性能。The straw fiber raw material used in the present invention selects the mixing of long straw fibers and short fibers, in order to mix the straw fibers and the inorganic adhesive evenly, so as to promote the compact structure of the board and improve the mechanical properties of the board. The long straw fibers in the board overlap each other to form a network structure interwoven vertically and horizontally, which can inhibit the generation and spread of micro-cracks in the inorganic gel system, improve the elastic modulus of the board, and at the same time retain the natural shape of the straw; The fiber has a large specific surface area and is more easily infiltrated by the water-soluble silicon source. After mixing evenly, it is filled inside the board to improve the internal bonding strength of the board, thereby effectively improving the mechanical properties of the board.

为了实现上述技术方案,本发明所述秸秆气凝胶难燃保温板的制备步骤如下:In order to realize the above technical solution, the preparation steps of the straw aerogel flame-retardant insulation board of the present invention are as follows:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长短不同的纤维细丝,筛分后获得所需的秸秆长纤维和秸秆短纤维,长短纤维按比例复配,成为秸秆原料;(1) After the straw is dedusted, it is dried, and subjected to mechanical grinding to obtain fiber filaments of different lengths. After screening, the required long straw fibers and short straw fibers are obtained, and the long and short fibers are compounded in proportion to become straw raw materials;

(2)首先按比例称量水溶性硅源、钙源、步骤(1)秸秆原料、聚乙烯醇及水,其次将水溶性硅源与水配置成水溶液,最后将秸秆原料依次与聚乙烯醇、水溶性硅源溶液、钙源搅拌,混合均匀后,获得混合物料;(2) First, weigh the water-soluble silicon source, calcium source, step (1) straw raw material, polyvinyl alcohol and water in proportion, secondly prepare the water-soluble silicon source and water into an aqueous solution, and finally mix the straw raw material with polyvinyl alcohol in sequence , the water-soluble silicon source solution and the calcium source are stirred and mixed to obtain a mixed material;

(3)将步骤(2)的混合物料经铺装预压成型、高温高压固型后得到秸秆气凝胶难燃保温板的板坯;(3) obtaining the slab of the straw aerogel flame-retardant thermal insulation board after the mixed material of step (2) is pre-pressed by paving and solidified at high temperature and high pressure;

(4)步骤(3)得到板坯经过养护、裁边,砂光处理后,获得本发明所述秸秆气凝胶难燃保温板成品板。(4) Step (3) After curing, trimming, and sanding the slab obtained in step (3), the finished straw aerogel flame-retardant thermal insulation board according to the present invention is obtained.

步骤(1)中所述机械磨解后的秸秆纤维长度不大于2cm。The length of the mechanically ground straw fibers in step (1) is not more than 2 cm.

步骤(3)中所述预压成型的操作条件为常温常压,压至板坯成型即可。The operating conditions of the pre-compression molding in step (3) are normal temperature and normal pressure, and it can be pressed until the slab is formed.

本发明有益效果如下:The beneficial effects of the present invention are as follows:

(1)本发明所述的秸秆气凝胶难燃保温板既保留了秸秆的天然纹理,具有较好的装饰效果,也具有轻质高强、表面平整、难燃的技术特征,有利于推动秸秆的资源化利用。(1) The straw aerogel flame-retardant insulation board of the present invention not only retains the natural texture of the straw, has a good decorative effect, but also has the technical characteristics of light weight, high strength, smooth surface, and flame resistance, which is conducive to promoting the straw resource utilization.

(2)本发明所述的秸秆气凝胶难燃保温板能够达到B1级阻燃,具有轻质无醛、隔热隔音和防霉防蛀等特点。(2) The straw aerogel flame-retardant insulation board of the present invention can reach B1 level flame-retardant, and has the characteristics of light weight, no formaldehyde, heat insulation, sound insulation, mildew and moth resistance, and the like.

(3)采用本发明所述组分在高温高压条件下制备板材,有利于降低板材密度,提高板材保温性能;(3) Using the components of the present invention to prepare the board under high temperature and high pressure conditions is conducive to reducing the density of the board and improving the thermal insulation performance of the board;

(4)本发明采用长短纤维复配的秸秆纤维原料填充于板材内部,使秸秆纤维与无机胶黏剂混合均匀,从而提高板材的内胶合强度,从而能有效地提高板材的力学性能。(4) The present invention uses long and short fiber composite straw fiber raw materials to fill the interior of the board, so that the straw fiber and the inorganic adhesive are evenly mixed, thereby improving the internal bonding strength of the board, thereby effectively improving the mechanical properties of the board.

附图说明Description of drawings

图1为本发明实施例1中制备的保温板表面结构示意图。FIG. 1 is a schematic diagram of the surface structure of the thermal insulation board prepared in Example 1 of the present invention.

具体实施方式Detailed ways

下面对本发明实施例中的技术方案进行清楚、完整地描述。显然,所描述的实施例是本发明一部分实施例。而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the present invention. not all examples. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

实施例1Example 1

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照2:8的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long and different fiber filaments. After screening, long fibers with a length of 1 to 2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 2:8 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠370g、石膏150g、聚乙烯醇6g、水420g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 370g of sodium silicate, 150g of gypsum, 6g of polyvinyl alcohol, and 420g of water, respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source, and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于180℃,3MP的热压机上定厚0.9cm,热压固型12min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material is placed in a 55cm×55cm mold and formed, and then placed on a 180°C, 3MP hot press to set a thickness of 0.9cm, and hot-pressed for 12 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

图1为实施例1制备的保温板表面结构示意图,由图中可以发现该板材表面平整同时保留了秸秆的天然纹理。FIG. 1 is a schematic diagram of the surface structure of the thermal insulation board prepared in Example 1. From the figure, it can be found that the surface of the board is flat while retaining the natural texture of straw.

实施例2Example 2

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照2:8的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long and different fiber filaments. After screening, long fibers with a length of 1 to 2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 2:8 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠200g、石膏120g、聚乙烯醇5g、水260g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 200g of sodium silicate, 120g of gypsum, 5g of polyvinyl alcohol, and 260g of water respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于160℃,7MP的热压机上定厚0.9cm,热压固型30min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material is placed in a 55cm×55cm mold and formed, and then placed on a 160°C, 7MP hot press to set a thickness of 0.9cm, and hot-pressed for 30 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

实施例3Example 3

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照2:8的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long and different fiber filaments. After screening, long fibers with a length of 1 to 2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 2:8 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠370g、石膏150g、聚乙烯醇6g、水420g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 370g of sodium silicate, 150g of gypsum, 6g of polyvinyl alcohol, and 420g of water, respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source, and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于220℃,3MP的热压机上定厚0.9cm,热压固型8min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material is placed in a 55cm×55cm mold and formed, and then placed on a 220°C, 3MP hot press to set a thickness of 0.9cm, and hot-pressed for 8 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

实施例4Example 4

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照3:7的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long and different fiber filaments. After screening, long fibers with a length of 1-2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 3:7. 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠370g、石膏150g、聚乙烯醇6g、水420g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 370g of sodium silicate, 150g of gypsum, 6g of polyvinyl alcohol, and 420g of water, respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source, and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于180℃,3MPa的热压机上定厚0.9cm,热压固型12min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material was placed in a 55cm×55cm mold and formed, and then placed on a 180°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 12 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

实施例5Example 5

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照3:7的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long and different fiber filaments. After screening, long fibers with a length of 1-2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 3:7. 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠400g、石膏150g、聚乙烯醇6g、水440g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 400g of sodium silicate, 150g of gypsum, 6g of polyvinyl alcohol, and 440g of water, respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source, and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于180℃,3MPa的热压机上定厚0.9cm,热压固型12min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material was placed in a 55cm×55cm mold and formed, and then placed on a 180°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 12 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

实施例6Example 6

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照3:7的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long and different fiber filaments. After screening, long fibers with a length of 1-2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 3:7. 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠370g、石膏150g、聚乙烯醇12g、水420g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 370g of sodium silicate, 150g of gypsum, 12g of polyvinyl alcohol, and 420g of water, respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source, and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于180℃,3MPa的热压机上定厚0.9cm,热压固型12min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material was placed in a 55cm×55cm mold and formed, and then placed on a 180°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 12 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

实施例7Example 7

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照1:9的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long fibers with different lengths. After screening, long fibers with a length of 1 to 2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 1:9 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠370g、石膏120g、聚乙烯醇6g、水420g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 370g of sodium silicate, 120g of gypsum, 6g of polyvinyl alcohol, and 420g of water, respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source, and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于180℃,3MPa的热压机上定厚0.9cm,热压固型12min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material was placed in a 55cm×55cm mold and formed, and then placed on a 180°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 12 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

实施例8Example 8

本发明所述秸秆气凝胶难燃保温板的制备方法,包括如下步骤:The preparation method of the straw aerogel flame-retardant thermal insulation board according to the present invention comprises the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,长短纤维按照3:7的比例配合,称量1000g秸秆原料;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long and different fiber filaments. After screening, long fibers with a length of 1-2 cm and short fibers with a length of less than 1 cm are obtained. The long and short fibers are 3:7. 1000g of straw raw materials were weighed;

(2)分别称量硅酸钠370g、石膏150g、聚乙烯醇6g、水420g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 370g of sodium silicate, 150g of gypsum, 6g of polyvinyl alcohol, and 420g of water, respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source, and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于200℃,3MPa的热压机上定厚0.9cm,热压固型10min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material is placed in a 55cm×55cm mold and formed, and then placed on a 200°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 10 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

对比例1(不加钙源)Comparative Example 1 (without calcium source)

一种秸秆气凝胶难燃保温板的制备方法,包括如下步骤:A preparation method of a straw aerogel flame-retardant thermal insulation board, comprising the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,称量1000g稻秸短纤维;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long fibers of different lengths. After sieving, long fibers with a length of 1-2 cm and short fibers with a length of less than 1 cm are obtained. fiber;

(2)分别称量硅酸钠370g、聚乙烯醇6g、水420g,秸秆纤维依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) respectively weighing 370 g of sodium silicate, 6 g of polyvinyl alcohol, and 420 g of water, and stirring the straw fibers with the polyvinyl alcohol solution, the water-soluble silicon source and the calcium source in turn, and after mixing uniformly, a mixed material was obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于180℃,3MPa的热压机上定厚0.9cm,热压固型8min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material was placed in a 55cm×55cm mold and formed, and then placed on a 180°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 8 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

对比例2(稻秸全部采用短纤维)Comparative example 2 (the rice straw is all short fiber)

一种秸秆气凝胶难燃保温板的制备方法,包括如下步骤:A preparation method of a straw aerogel flame-retardant thermal insulation board, comprising the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获长度小于1cm的短纤维,称量1000g秸秆短纤维原料;(1) After the straw is dedusted, it is dried, and subjected to mechanical grinding to obtain different long fiber filaments. After sieving, short fibers with a length of less than 1 cm are obtained, and 1000 g of straw short fiber raw materials are weighed;

(2)分别称量硅酸钠370g、聚乙烯醇6g、水420g,秸秆原料依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) Weighing 370g of sodium silicate, 6g of polyvinyl alcohol, and 420g of water respectively, the straw raw material is stirred with polyvinyl alcohol solution, water-soluble silicon source and calcium source in turn, and after mixing uniformly, a mixed material is obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于180℃,3MPa的热压机上定厚0.9cm,热压固型8min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material was placed in a 55cm×55cm mold and formed, and then placed on a 180°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 8 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

对比例3(降低温度)Comparative Example 3 (reduce the temperature)

一种秸秆气凝胶难燃保温板的制备方法,包括如下步骤:A preparation method of a straw aerogel flame-retardant thermal insulation board, comprising the following steps:

(1)秸秆除尘后,烘干处理,经机械磨解,获得长段不同的纤维细丝,筛分后获得长度1~2cm的长纤维和长度小于1cm的短纤维,称量1000g稻秸短纤维;(1) After the straw is dedusted, it is dried and decomposed by mechanical grinding to obtain long fibers of different lengths. After sieving, long fibers with a length of 1-2 cm and short fibers with a length of less than 1 cm are obtained. fiber;

(2)分别称量硅酸钠370g、聚乙烯醇6g、水420g,秸秆纤维依次与聚乙烯醇溶液、水溶性硅源、钙源搅拌,混合均匀后,获得混合物料;(2) respectively weighing 370 g of sodium silicate, 6 g of polyvinyl alcohol, and 420 g of water, and stirring the straw fibers with the polyvinyl alcohol solution, the water-soluble silicon source and the calcium source in turn, and after mixing uniformly, a mixed material was obtained;

(3)混合物料置于55cm×55cm的模具中铺装成型,再置于120℃,3MPa的热压机上定厚0.9cm,热压固型8min,制秸秆气凝胶难燃保温包的板坯;(3) The mixed material is placed in a 55cm×55cm mold and formed, and then placed on a 120°C, 3MPa hot press to set a thickness of 0.9cm, and hot-pressed for 8 minutes to make a straw aerogel flame retardant thermal insulation package. blank;

(4)板坯在室温下养护3天后、裁边,砂光,获得成品板。(4) After curing the slab at room temperature for 3 days, trimming and sanding to obtain a finished slab.

性能测试Performance Testing

对本发明各实施例及对比例得到的板材进行性能测试,其结果见表1所示。The performance tests were carried out on the sheets obtained by the embodiments of the present invention and the comparative examples, and the results are shown in Table 1.

表1难燃木质基板的性能测试结果Table 1 Performance test results of flame-retardant wood substrates

Figure BDA0003697888490000081
Figure BDA0003697888490000081

Figure BDA0003697888490000091
Figure BDA0003697888490000091

由表1中各实施例及对比例的抗折强度及抗压强度的数据可以发现,本发明各实施例中,长纤维保留了秸秆的宏观力学性能,适当提高长纤维的含量,有利于板材力学性能的提升。From the data of flexural strength and compressive strength of each embodiment and comparative example in Table 1, it can be found that in each embodiment of the present invention, the long fibers retain the macroscopic mechanical properties of straw, and the content of long fibers is appropriately increased, which is beneficial to the board. Improved mechanical properties.

由表1可以看出,适当提高温度,有利于样板力学性能的提升。同时高温下,有机质中木材脱水缩合,使样板的耐水性有所提升,表现为样板的吸水厚度膨胀率下降。It can be seen from Table 1 that an appropriate increase in temperature is beneficial to the improvement of the mechanical properties of the sample. At the same time, at high temperature, the wood in the organic matter is dehydrated and condensed, which improves the water resistance of the sample, which is manifested as a decrease in the expansion ratio of the water absorption thickness of the sample.

由表1中数据可以发现,实施例4、5可以看出,适当提高硅钙比(提高硅酸钠含量,降低石膏含量),有利于无机料的强度相晶体从水合C-S-H晶型转变为结晶度更高的托贝莫来石晶体,从而有利于板材力学性能的提升。It can be found from the data in Table 1 that it can be seen in Examples 4 and 5 that appropriately increasing the ratio of silicon to calcium (increasing the content of sodium silicate and reducing the content of gypsum) is conducive to the transformation of the strength phase crystal of the inorganic material from the hydrated C-S-H crystal form into a crystal. A higher degree of tobermorite crystal, which is beneficial to the improvement of the mechanical properties of the sheet.

实施例6、8可以看出,提高温度可以促进秸秆中半纤维素、木质素的玻璃化转变程度,促进纤维素气凝胶的形成,有利于羟基的脱水缩合反应,提高板材的疏水性。It can be seen from Examples 6 and 8 that increasing the temperature can promote the glass transition of hemicellulose and lignin in the straw, promote the formation of cellulose aerogel, facilitate the dehydration condensation reaction of hydroxyl groups, and improve the hydrophobicity of the board.

对比例1和实施例1可以看出,钙源作为硅源的固化剂,能够在高温高压的条件下与形成水合硅酸钙晶体,从而提高板材的力学性能,失去钙源,板材的力学性能下降明显。It can be seen from Comparative Example 1 and Example 1 that calcium source, as a curing agent for silicon source, can form hydrated calcium silicate crystals under high temperature and high pressure conditions, thereby improving the mechanical properties of the plate, losing the calcium source and reducing the mechanical properties of the plate. decreased significantly.

对比例1和实施例2可以看出,长短纤维的搭接方式能有效地提高板材的力学性能,同时降低板材的吸水厚度膨胀率,减轻板材的掉渣问题。It can be seen from Comparative Example 1 and Example 2 that the overlapping method of long and short fibers can effectively improve the mechanical properties of the board, reduce the water absorption thickness expansion rate of the board, and reduce the slag problem of the board.

对比例3和实施例1可以看出,温度较低(120℃)时,秸秆内部的木质素和半纤维素玻璃化转变程度不够,形成的纤维素气凝胶强度较弱,从而影响保温板的力学性能和保温性能。同时,低温(120℃)时,硅源和钙源生成富钙的C-S-H凝胶,140℃时生成低结晶度的托贝莫来石晶体,在180~200℃时逐步转化为形成结晶度良好的托贝莫来石晶体。It can be seen from Comparative Example 3 and Example 1 that when the temperature is low (120°C), the glass transition degree of lignin and hemicellulose inside the straw is not enough, and the strength of the formed cellulose aerogel is weak, thus affecting the insulation board. mechanical properties and thermal insulation properties. At the same time, at low temperature (120 °C), the silicon source and calcium source generate calcium-rich C-S-H gel, and at 140 °C, low-crystallinity tobermorite crystals are formed, and at 180-200 °C, it gradually transforms to form a good crystallinity. of tobermorite crystals.

Claims (10)

1. The utility model provides a straw aerogel fire-retardant heated board which characterized in that: uniformly mixing straw raw materials, a coupling agent, an inorganic material and water, paving, prepressing, forming, and then solidifying at high temperature and high pressure to obtain the straw composite material; the inorganic material comprises a water-soluble silicon source and a calcium source;
the weight parts of the components are as follows:
Figure FDA0003697888480000011
the mass ratio of the water to the inorganic material is 0.8-1;
the technological parameters of the high-temperature high-pressure solid mold are as follows: the temperature is 160-220 ℃, the unit pressure is 3-10 MPa, and the setting time is 10-30 min;
the straw raw material is formed by compounding long straw fibers and short straw fibers;
the length of the long straw fibers is 1-2 cm, and the length of the short straw fibers is less than 1 cm.
2. The straw aerogel flame-retardant insulation board as claimed in claim 1, wherein the straw raw material comprises 10-30% by mass of straw long fibers and 70-90% by mass of straw short fibers.
3. The straw aerogel flame-retardant insulation board according to claim 1 or 2, wherein the moisture content of the straw raw material is less than 10 wt%.
4. The straw aerogel flame-retardant insulation board according to claim 1, wherein the coupling agent is polyvinyl alcohol.
5. The straw aerogel flame-retardant insulation board according to claim 1, wherein the water-soluble silicon source is instant powdery sodium silicate, and the modulus is 2.1-3.4.
6. The straw aerogel flame-retardant insulation board according to claim 1, wherein the calcium source is semi-hydrated gypsum.
7. The preparation method of the straw aerogel flame-retardant insulation board as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
(1) after the straw is dedusted, drying, mechanically grinding to obtain fiber filaments with different lengths, screening to obtain the required long fibers and short fibers of the straw, and compounding the long fibers and the short fibers in proportion to obtain the straw raw material;
(2) firstly, weighing a water-soluble silicon source, a calcium source, the straw raw material in the step (1), polyvinyl alcohol and water in proportion, preparing the water-soluble silicon source and the water into an aqueous solution, and finally stirring the straw raw material, the polyvinyl alcohol, the water-soluble silicon source solution and the calcium source in sequence to obtain a mixed material after uniform mixing;
(3) paving, prepressing and molding the mixed material obtained in the step (2), and solidifying at high temperature and high pressure to obtain a plate blank of the straw aerogel flame-retardant insulation board;
(4) and (4) maintaining, cutting edges and sanding the plate blank obtained in the step (3) to obtain the straw aerogel flame-retardant insulation board finished product plate.
8. The preparation method of the straw aerogel flame-retardant insulation board according to claim 7, wherein the length of the straw fiber after mechanical grinding in the step (1) is not more than 2 cm.
9. The preparation method of the straw aerogel flame-retardant insulation board according to claim 7, wherein the solid content of the water-soluble silicon source solution in the step (2) is 30-40%.
10. The preparation method of the straw aerogel flame-retardant insulation board according to claim 7, wherein the pre-pressing molding in the step (3) is performed under normal temperature and normal pressure until a board blank is molded.
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CN117209246B (en) * 2023-10-19 2024-06-21 江苏宇航板业有限公司 Production process of silica-calcium gel water-absorbing foot pad

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Denomination of invention: Straw aerogel flame retardant insulation board and its preparation method

Granted publication date: 20230718

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